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Studies on Nano Cellulose Century Fiber Composites

International Journal of Trend in Scientific Research and Development (IJTSRD)
International Open Access Journal | www.ijtsrd.com
ISSN No: 2456 - 6470 | Volume - 2 | Issue – 6 | Sep – Oct 2018
Studies on Nano Cellulose Century Fiber Composites
C. Shashikanth1, D. K. Nageswara Rao2
Assistant Professor
Professor, Mechanical Engineering, 2Professor
Malla Reddy College of Engineering, Hyderabad, Telangana, India
Nano cellulose composites are used for advanced
applications for structural parts and electronic
components. Biocompatible water soluble cellulose
composites are used in medical applications
ications as well.
Nano cellulose fibers are extracted through various
chemical and mechanical treatments to separate the
cellulose and to further refine it. Composites are made
using thermosetting polyester resin and biodegradable
poly vinyl (PVA). A research
rch work is proposed in this
paper for extraction of lignocellulose and nano
cellulose fibers from century plant and developing the
composites for evaluation of TGA, DSC, DMA,
dielectric, tensile, flexural, impact, hardness and
hygroscopic properties.
lications for the
composites will be suggested based on the the
properties of the composites.
Keyword: Century fiber composites; nanocellulose
fibers; nano cellulose composites; biodegradable
cellulose composites have drawn the attention
of the researchers for development thermosetting and
biodegradable materials for automotive, packaging
and medical applications [1-10].
10]. Nano cellulose fiber
composites are fully biodegradable and biocompatible
with excellent mechanical properties. Due to high
crystallinity and high aspect ratio and low density of
the nano cellulose fibers, there is considerable
increase in the stiffness of the composites produced.
The comparative study [1-3] of mechanical, thermal,
electrical and water absorption properties of different
natural fiber composites has identified that the
Century fiber has great potential to give better
properties. There has been an increasing interest on
use of natural fiber composites over the last decade
and extensive research has been carried out to explore
the best properties for various applications [4, 5].
Nano cellulose fibers are isolated from a variety of
natural fibers by chemical and mechanical treatments
[5]. Chemical treatments prior to mechanical
treatments reduce
uce the size of the fibers before
homogenization by [6] and reduce the energy
consumption during mechanical treatments. Different
chemical treatments include: alkaline treatment
coupled with high pressure defibrillation, acid
treatment, enzyme-assisted
assisted hydrolysis and acid
hydrolysis. Mechanical treatments include: high
cryocrushing and grinding. Isolation of nano fibers is
assisted by oxidation pretreatment by 2Tetramethylpiperidine-1-oxyl
facilitates. Other methods include
clude steam explosion and
electro- spinning [7-11].
11]. Nano fibrillated cellulose
(NFC) reinforced composites are produced using
phenolic resin.
pectin polyurethane,
Styrene butyl acryl ate amyl pectin,
melamine formaldehyde, etc. Nano composites are
made by hand layup technique using bio-based
resin and TEMPO oxidized NFC. The specimens are
investigated for mechanical,, dynamic mechanical,
thermal [12] and dielectric properties as well as
humidity absorption, morphology and transparency of
the composites [6]. Different
ifferent biodegradable polymers
used are: PEO-poly
poly (ethylene oxide), PVA-poly
(vinyl alcohol), and PAA- poly
PCL-poly (ε-caprolactone), PLAPLA poly (lactic acid),
PS-polystyrene, EVOH-ethylene
copolymer, PMMA-poly (methyl
methyl methacrylate) [12,
]. Thermoplastic rice straw nano cellulose
composites are made using reinforced starch polymer
[15]. In the first step, almost all the non-cellulosic
components are removed from the straw and a white
pulp of cellulosic fibers are obtained.
Then a diluted
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International Journal of Trend in Scientific Research and Development (IJTSRD) ISSN: 2456-6470
suspension of fibers was ultra-sonicated
sonicated to destroy
inter molecular hydrogen bonds and nano fiber
networks are obtained. The fibers are then used for
casting films of the composite. It was found that the
yield strength and Young‘s modulus of the nano
composites is due to the reinforcement by cellulose
fibers. Humidity Absorption resistance
significantly enhanced.
Recently, modified cellulose has been used as
reinforcement for various composites with water
soluble polymers. Addition of cellulose increased the
viscosity and mechanical properties and accelerated
the rate of biodegradation. Chemical modification of
cellulose has been an important route for the
production of multifunctional materials. High strength
biodegradable composite films for membrane and
packaging applications are developed by film casting
method using modified cellulose with poly(vinyl
alcohol) in different
erent compositions [8,15,16]. These
films are characterized for mechanical, moisture
absorption, gas barrier, and biodegradable properties
[16,17]. They have shown good transparency,
flexibility, good mechanical and biodegradable
properties. These films have
ve exhibited better barrier
properties with increase in percentage of modified
cellulose. Literature review revealed that reported
research has not been found on Century cellulose nano
fiber composites. Century fibers will be extracted from
Agave Americana plants are abundantly available as
border plant. The century fibers are widelyused in the
textile and paper industry.
The century
cellulose fibers will be used to cast various structural
parts in Automobiles,, electronic and packaging
The proposed research work is to produce wealth
from waste by developing useful products from desert
plants. By extracting nano cellulose fibers from leaves
of Century plant. Century nano cellulose fiber sheets
are molded using thermoset polyester
er resin and also
poly (vinyl alcohol), a biodegradable resin.
The composites will be tested for various mechanical
properties such as: flexural, tensile, fracture, impact,
Barcol hardness and water absorption and dielectric
breakdown properties. Thermal properties
roperties like, glass
transition temperature and thermal degradation will be
studied using Differential Scanning Calorimetry and
Thermogravimetric Analysis respectively. Scanning
Electron Microscopy will be done to study the
fracture behavior of the composite.
Based on the
results of the studies, the scope of application of the
material will be suggested.
A. Century Plant
Century (Agave Americana) plant belongs to
Agavaceae family and is native to Mexico and its
namee is derived referring to the long time it takes to
flower. These plants grow in clusters and are
generally used for fencing. Their leaves are 2 m long
and 25 cm wide. They are located as a rosette without
trunk. Century fiber has drawn attention by several
researchers because of their large leaf length, leaf
biomass, fiber length, fineness, density and high
B. Extraction of Century Fibers
The lignocellulosic fibers from Century plant are
produced from leaves by retting process. The leaves
are cut and dried to allow the watery substance to
evaporate and then soaked in still water for 15 days.
The fermented soft greenish substance is washed
thoroughly and the fibers are peeled off the leaves and
are washed and dried in shady place. The length of
the fibers is between 100-123
123 cm and the size ranges
between 150µ m to 300 µm.
C. Extraction of Cellulose [16,17]
Cellulose is extracted by a process called water prepre
hydrolysis [10]. The fibers which are of 1-1.25
m long
are cut into approximate length of 5-10mm.
chopped fibers are dewaxed where a mixture of
Toulene/ethanol (2:1 vol/vol) is poured in flask and
the fibers were put in a cloth and placed in the Soxhlet
extractor and boiled at a temperature of 70°C for 6
hours. They are washed with ethanol for
f 30 min and
then allowed to dry. The de-waxed
fibers are then
mixed with 0.1M NaOH in 50% volume of ethanol at
45°C for 3 hours under continuous stirring by keeping
the beaker on a magnetic stirrer. Then the fibers are
treated with H2O2 at pH=10.5(buffer solution) is
carried out at 45°C in a solution of H2O2with
different concentrations, viz., (a)0.5% H2O2 (b)1%
H2O2 (c)2% H2O2 (d)3% H2O2 for 3 hours each
under continuous agitation. Then each mixture is
treated with 10% w/v NaOH + 1% w/v
Na2B4O7.10H2O at 32°C for 15 hours under
continuous stirring. Then, solid obtained will be
filtered off. Salt formation will be confirmed by
solubility test, since it is freely soluble in water. This
@ IJTSRD | Available Online @ www.ijtsrd.com | Volume – 2 | Issue – 6 | Sep-Oct
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International Journal of Trend in Scientific Research and Development (IJTSRD) ISSN: 2456-6470
salt will be treated with 2-(Trifluromethyl)
benzoylchloride in the presence of pyridine as a base
cum Solvent and stirred overnight at 100◦C.
At the end of the process, only cellulose will be left
which is then washed with 95% ethanol and then
water and dried at 60°C in an oven until the weight
remains constant. Then the fibers are ground to obtain
in the form of a powder. Important stages aare
illustrated in Fig. 1.
Fig.1. Different stages of extraction of nano cellulose
D. Casting of Biodegradable Composite Films[9]
benzoylchloride will be taken in water along
acetonitrile as purifying solvent and Poly(vinyl
alcohol) as matrix in different proportions as: 10 : 90,
20 : 80, 30 : 70, 40 : 60, 50 : 50, 60 : 40, 70 : 30, 80 :
20, 90 : 10, and 95 : 05 ratios. The reaction mixture
was heated to 100◦C
C for 24 hrs. After 24 hrs, the
reaction mass will turn to viscous state, it will be
allowed to reach room temperature and spread on the
Teflon mold of one square feet with 3mm depth. The
mold will be coated with mold releasing spray and
dried under vacuum oven at 100◦C to remove water
contents completely. After complete drying of the cast
films, they are stored in moisture free environment.
and Engineering Instruments, New Delhi, at a cross
head speed of 1.25 mm/minute, at standard laboratory
atmosphere of 23°C ± 2°C (73.4°F ± 3.6°F) and 50 ±
5 percent relative humidity. Specimens for flexural
test are cut from laminas as per ASTM D790.
Flexural Strength: Flexural strength is the maximum
stress in the outer surface of the specimen at the
moment of break. When the homogeneous elastic
material is tested with threethree point system, the
maximum stress occurs at the midpoint.
Flexural Modulus: Flexural modulus (N/m2) is the
ratio off flexural stress to the strain in flexural
deformation.It is a measure of the stiffness during the
initial part of the bending process. Flexural modulus
is the ratio of stress to corresponding strain within the
elastic limit.
Fig.2. Flexural Test Setup
A. Preparation of Specimens and Testing
Preparation of specimens for flexural test tensile ttest
Impact test hardness, moisture absorption test will be
done as per corresponding ASTM standards. For
morphology studies, Scanning Electron Microscope
(SEM) was used.
B. Flexural test, flexural strength, flexural
The flexural strength (N/m2) of a material is defined
as the ability to resist deformation under transverse
loads. Flexural properties will be evaluated as per
ASTM D-790-03 through three-point
point bend test on
compression testing machine supplied by Hydraulic
Fig.3. Universal Testing Machine Zwick/Roell Z010
C. Tensile test, tensile strength and tensile
Tensile Strength: It is the maximum stress (N/m2) that
the material can withstand before failure. It is also
called as ultimate tensile strength.
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International Journal of Trend in Scientific Research and Development (IJTSRD) ISSN: 2456-6470
Tensile Modulus: It is also known as Young‘s
modulus (N/m2) or modulus of elasticity and is a
measure of the stiffness of the material. It is given by
the ratio of the uniaxial stress to the uniaxial strain.
Tensile test will be conducted on an electronic tens
testing machine Zwick/Roell Z010-10KN
10KN-UTM at a
cross head speed of 3 mm/min and gauge length of 50
mm. Standard Type IV dumb bell shaped specimens
are used as per ASTM D-638-03.
03. The values of tensile
strength and tensile modulus are obtained from the
deflection values by taking the maximum load
resisted by the specimen up to the point of fracture
and the corresponding strain. Loading of the specimen
on the Tensile Testing Machine and the grips used for
holding the specimen are shown in Figs. 3.
D. Impact strength
It is the ability of the material to withstand shock
loading. It is measured by the work done (kJ/m2) in
fracturing the material under shock loading. Izod
impact test is used in the present case. Notched impact
performance of the composite is evaluated as per
ASTM D-256-05
05 using Pendulum impact tester,
model IT 30 Izod impact supplied by PSI Sales Pvt.
Ltd., New Delhi, shown in Fig. 4. The size of the
samples is 12 mm X 60mm. The test specimen is
supported by a vertical cantilever beam and the
specimen was broken by the swing of the pendulum.
The energy absorbed in doing so is measured as
difference between the height of drop before rupture
and the height of rise after rupture of the test specimen.
Fig.5. Barcol Hardness Tester
F. Scanning Electron Microscopy(SEM)
The morphology of fractured surfaces of the
composites will be studied by Scanning Electron
Microscopy (SEM) using EVOMA15 Smart
shown in Fig. 6. The fracture behavior of the material
indicates the amount of energy absorbed before
fracture, which is a measure of toughness of the
material. The SEM reveals the nature of the bond
between the fibers and the matrix.
rming SEM, The fractured specimens
Before performing
will be placed on a stub as shown in Fig. 7 coated with
platinum and inserted into the scanning barrel. The
inter-condition of the scanning barrel is vacuumed to
prevent interference of scanning picture due to the
presence of air. Magnification, focus, contrasts and
brightness of the result is adjusted to produce the best
E. Barcol Hardness
Barcol hardness test characterizes
racterizes the indentation
hardness of the materials through the depth of
penetration of an indenter, often used for composite
materials. Standard test method ASTM D
D-2583-75 is
used to find indentation hardness of the composite
through Barcol impresser model
no. 934-1 shown in Fig. 5.
Fig.6. EVOMA15 Smart SEM
Fig.4. Pendulum Impact Tester
Fig.7. Stub of the EVOMA15 Smart SEM
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International Journal of Trend in Scientific Research and Development (IJTSRD) ISSN: 2456-6470
G. Differential Scanning Calorimetry(DSC)
Glass transition temperature Tg of a non
material is the critical temperature at which the
material changes its behavior from hard and brittle to
rubbery state. This is less than the melting
temperature (Tm). Differential Scanning Calorimetry
is used for finding the Tg of the composites.
omposites. DSC is
performed with the help of Mettler using Star SW 8.1
analyzer to measure Tg. The temperature is
programmed in the range of 25°-300°C
300°C with a heating
rate of 10°C/min in nitrogen atmosphere with a flow
rate of 30 ml/min. The Mettler DSC ins
instrument and
the silver pan used for conducting the test are shown
in Figs. 9.
thermocouple. Temperature is measured and
controlled by a thermocouple assembly under the
sample pan.
I. Dynamic Mechanical Analysis(DMA)
This analysis gives the storage modulus, loss modulus
and damping property of the materials. Material‘s
response for stress, temperature and frequency is
determined through this test. Dynamic Mechanical
Analysis, otherwise known as DMA, is a technique
where a small deformation is applied to a sample in a
cyclic manner. This allows the materials response
stress, temperature, frequency and other values to be
studied. The term is also used to refer to the analyzer
that performs the test. DMA is also called DMTA for
Dynamic Mechanical Thermal Analysis. Specimens
for dynamic mechanical analysis are prepared as per
ASTMD 4065.
The Pyris Diamond DMA equipment by Perkin-Elmer
Instruments is shown in Fig. 10. DMA yields
information about the mechanical properties of a
specimen placed under minor sinusoidal oscillating
force and temperature.
Figure 8 Mettler DSC Instrument
Fig.10.. Pyris Diamond DMA
Fig.9. Thermo gravimetric Analyzer Perkin
H. Thermo gravimetric Analysis (TGA)
Thermal degradation or weight loss due to heating is a
re of the thermal stability of the material under
high temperature. Thermo gravimetric analysis (TGA)
curves are used to determine the thermal degradation
and thermal stability of the polymeric material.
Thermal decomposition is observed as per ASTM E
1131 in terms of loss of global mass using TA
Instrument TGAQ50 V20.10 Build 36 thermo
gravimetric analyzer shown in Fig.9. The sample area
is enclosed by a cylinder inside of the quartz tube.
This energy-absorbing
absorbing cylinder absorbs radiation
from the lamps and heats
eats the sample, pan, and
Fig.11. Hot air oven
J. Dielectric Strength
It is a measure of the electrical resistance of the
material given by the maximum voltage that an
insulating material can withstand before it
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International Journal of Trend in Scientific Research and Development (IJTSRD) ISSN: 2456-6470
decomposes or becomes a conducting material by
losing its insulation property. The test is conducted as
per ASTM D149: Standard Test Method for Dielectric
Breakdown Voltage and Dielectric Strength of Solid
Electrical Insulating Materials at Commercial Power
Frequencies. Voltage at a commercial power
cy 60 hertz is applied to a test specimen. The
voltage is increased from zero, until the dielectric
failure of the test specimen occurs. Hipotronics 715
715-1A AC Dielectric Test set up will be used.
K. Water Absorption
Moisture absorption, soluble matter lost and long term
immersion properties are evaluated. Water absorption
tests are conducted on rectangular specimens of 76.2 x
25.4 mm2 size shown in Fig. 18 as per ASTM D
D-57098. This test method covers the determination of the
relative rate of absorption of water by fiber when
immersed. The moisture content of a fiber is very
intimately related to such properties as electrical
insulation resistance, dielectric losses, mechanical
strength, appearance, and dimensions.
Short Time Immersion: The samples are conditioned
by heating in an oven at 50±3 oC for 24 hours and
then cooling to room temperature. The weights of the
samples will be taken by Shimadzu Electronic
Balance (AY 220) that has a readability of 0.001g. All
the samples are immersed in double distilled water for
24 hrs at room temperature. Reconditioning is done
by keeping them once again in the oven (Fig.11) for
24 hrs at 50±3 oC. Percentage increase in weight of
the specimen during immersion is obtained by the
ratio of increase in average weight of the conditioned
specimen after immersion in water for 24 hrs and the
average weight of reconditioned specimen is
calculatedd nearest to 0.01%. The amount of soluble
matter lost is given by the decrease in weight of the
specimen after reconditioning. The percentage of
water absorbed is the sum of the % increase in weight
and the soluble matter lost.
Long Term Immersion: The total
al water absorbed by
the conditioned specimens upon immersion for about
1200. The average % increase in weight of the
specimen is calculated. The percentage increase in
thickness or length or width swelling is obtained by
the ratio of the increase in the respective dimension
and the initial dimension.
The proposed research work on development of
Century nano cellulose polyester and PVA composites
can be of great value as new structural materials for
automobiles, electronic devices, and packaging
materials. The biodegradable PVA composites will
find applications as biocompatible materials.
Development of composites from these fibers will
contribute for the development of Green Technology.
Extraction of nano cellulose fibers from the plant
fiberss can grow as a cottage industry.
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